Sealing method for titanium-glass seal assembly

A technology of glass sealing and components, applied in metal material coating process, coating, solid-state diffusion coating, etc., can solve poor insulation resistance, poor performance stability of sealed products, poor wettability between titanium and titanium alloys and glass, etc. problems, to eliminate the formation of nitrides and oxides, improve production efficiency and yield, and avoid the effect of titanium alloy crystal phase transformation

Pending Publication Date: 2020-04-10
XIAN SEAL ELECTRONICS MATERIAL TECH CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires that the coefficient of thermal expansion between the metal and the glass is relatively matched, and the annealing process needs to be strictly controlled, so it has many shortcomings: 1) The fusion sealing process is difficult to control, and the process repeatability is poor, and the energy consumption is high; 2) ) The metals that can be used for sealing are limited to low-carbon steel, stainless steel and Kovar alloy, etc., and there are few types; 3) The performance and stability of the sealing product are poor due to the problem of process and material selection, and the sealing failure rate 4) The surface condition of the product after sealing is poor, causing great trouble to the subsequent surface treatment
[0004] However, there are many problems in the sealing process of titanium and titanium alloy materials, such as poor wettability with glass, high-temperature phase transition, etc., so it is difficult to achieve sealing with traditional glass. There are relatively serious defects in the alloy sealing interface. When disturbed by changes in the external environment, a large number of microcracks will be generated at the defects of the sealing interface, resulting in poor air tightness and poor insulation resistance.
At the same time, titanium and titanium alloys are easily oxidized at high temperatures, and different types of oxide layers are formed at different temperatures, which increases the difficulty of subsequent surface treatment
For this reason, the patent CN200810229958.2 proposes a titanium alloy sealing process, which needs to be sealed in an atmosphere of high-purity argon, and the temperature required for sintering the silicate system glass is as high as 960°C, but this The method does not solve the problem of poor wettability between titanium and titanium alloys and glass, and in the sealing process, an external abrasive tool is required for compression sealing. There is a big security risk in subsequent use

Method used

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  • Sealing method for titanium-glass seal assembly
  • Sealing method for titanium-glass seal assembly

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Pre-oxidize the metal shell at 300°C for 30 minutes, pre-oxidize the metal conductor stem at 300°C for 30 minutes, then put the metal shell, the glass body in the through hole of the metal shell, and the metal conductor stem into the sintering mold in the corresponding order In the process, put the semi-finished components together with the sintering mold into the high-temperature sintering furnace, introduce a mixture of 75% nitrogen and 25% hydrogen as a protective gas, raise the temperature to 750°C at 5°C / min, and keep it for 40 minutes for sintering to soften or melt A good tight seal is formed between the lower glass body, the metal conductor stem and the metal shell, and annealed at 5°C / min to 500°C for 15 minutes, and then lowered to room temperature at 10°C / min to obtain titanium-glass As for the sealing assembly, the formed titanium-glass sealing assembly is tested, and its performance parameters all meet the requirements for use.

Embodiment 2

[0044] Pre-oxidize the metal shell at 400°C for 20 minutes, pre-oxidize the metal conductor stem at 400°C for 20 minutes, then put the metal shell, the glass body in the through hole of the metal shell, and the metal conductor stem into the sintering mold in the corresponding order In the process, put the semi-finished components together with the sintering mold into the high-temperature sintering furnace, introduce a mixed gas of 90% nitrogen and 10% hydrogen as a protective gas, raise the temperature to 800°C at 15°C / min, and keep it for 25 minutes for sintering to soften or melt A good tight seal is formed between the glass body under the metal conductor core and the metal shell, and annealed at 15°C / min to 550°C for 10 minutes, and then cooled to room temperature at 15°C / min to obtain titanium- Glass sealed components.

Embodiment 3

[0046] Pre-oxidize the metal shell at 500°C for 10 minutes, pre-oxidize the metal conductor stem at 500°C for 10 minutes, then put the metal shell, the glass body set in the through hole of the metal shell, and the metal conductor stem into the sintering mold in the corresponding order In the process, put the semi-finished components together with the sintering mold into the high-temperature sintering furnace, introduce a mixed gas of 95% nitrogen and 5% hydrogen as the protective gas, raise the temperature to 880°C at 20°C / min, keep it for 15 minutes for sintering, and soften or melt the A good tight seal is formed between the glass body under the metal conductor core and the metal shell. It is annealed at 25°C / min to 550°C for 10 minutes, and then cooled to room temperature at 20°C / min to obtain excellent performance. Titanium-glass sealing components for aerospace connectors.

[0047] The titanium-glass sealing assembly prepared by the invention has excellent performance, a...

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Abstract

The invention discloses a sealing method for a titanium-glass seal assembly. A to-be-sealed titanium metal shell and metal conductor core column are respectively pre-oxidized at the temperature of 300-500 DEG C, so the wettability of metal and glass is improved, and the problem that the wettability of titanium and a titanium alloy with glass is poor is solved; a low-temperature oxidation layer isused as a protective layer to prevent the metal from being excessively oxidized at high temperature; the consistency of a sintered assembly is further ensured, and subsequent surface treatment is facilitated; a sealing mold provided with a sealing part into a sintering furnace for sintering; nitrogen and hydrogen binary atmosphere is introduced as protective gas; the formation of nitrides and oxides on the metal surfaces of titanium and the titanium alloy is eliminated, and the seal assembly surface treatment process is eliminated; the sintered sealing part is subjected to heat preservation atthe temperature of 500-550 DEG C so as to eliminate stress in the seal assembly, potential safety hazards in the using process of the seal assembly are eliminated, then the titanium-glass seal assembly can be obtained after the seal assembly is cooled to the room temperature, and the process is simple.

Description

technical field [0001] The invention belongs to a metal-glass sealing process, in particular to a sealing method for a titanium-glass sealing component. Background technique [0002] Traditional metal-glass sealing generally adopts a high-temperature fusion sealing method to fuse metal and glass together. This method requires that the coefficient of thermal expansion between the metal and the glass is relatively matched, and the annealing process needs to be strictly controlled, so it has many shortcomings: 1) The fusion sealing process is difficult to control, and the process repeatability is poor, and the energy consumption is high; 2) ) The metals that can be used for sealing are limited to low-carbon steel, stainless steel and Kovar alloy, etc., and there are few types; 3) The performance and stability of the sealing product are poor due to the problem of process and material selection, and the sealing failure rate 4) The surface state of the product after sealing is re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C27/02C23C8/10
CPCC03C27/02C23C8/10
Inventor 郝小军华斯嘉冯庆贾波杨文波刘卫红
Owner XIAN SEAL ELECTRONICS MATERIAL TECH CO LTD
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